CN114481366B - Preparation method of low-defect polyacrylonitrile-based carbon fiber - Google Patents
Preparation method of low-defect polyacrylonitrile-based carbon fiber Download PDFInfo
- Publication number
- CN114481366B CN114481366B CN202111415584.5A CN202111415584A CN114481366B CN 114481366 B CN114481366 B CN 114481366B CN 202111415584 A CN202111415584 A CN 202111415584A CN 114481366 B CN114481366 B CN 114481366B
- Authority
- CN
- China
- Prior art keywords
- temperature
- furnace
- low
- carbon fiber
- temperature carbonization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/32—Apparatus therefor
- D01F9/328—Apparatus therefor for manufacturing filaments from polyaddition, polycondensation, or polymerisation products
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses a preparation method of polyacrylonitrile-based carbon fiber with low structural defects. The method comprises the steps of unwinding a precursor, sequentially performing carbonization procedures such as a pre-oxidation furnace, a low-temperature carbonization furnace, a high-temperature carbonization furnace, surface treatment, washing, sizing, drying, winding and the like to obtain a finished carbon fiber, wherein the low-temperature carbonization furnace of the high-efficiency coke discharging system discharges low-temperature carbonized waste gas out of a furnace chamber more instantaneously and efficiently in the low-temperature carbonization process, so that the damage of byproducts such as tar and the like to the fiber is reduced; meanwhile, the high-temperature carbonization furnace is provided with a tow dehumidifying device, so that the damage of water vapor to fibers in the high-temperature carbonization process is reduced; finally, the preparation of the polyacrylonitrile-based carbon fiber with low structural defects is realized by combining the fine blending of the drafting at each stage in the carbonization process.
Description
Technical Field
The invention relates to the field of engineering production of high-performance polyacrylonitrile-based carbon fibers, in particular to a preparation method of low-defect polyacrylonitrile-based carbon fibers.
Background
The specific strength and specific modulus of the carbon fiber reinforced epoxy resin composite material are highest among the existing engineering materials. Along with the increasing maturity of application technology of the carbon fiber composite material in the fields of pressure vessels, aviation, aerospace and the like, the market demand for high-performance carbon fibers also presents a great increase, and especially the demand for high-performance polyacrylonitrile-based carbon fibers is most remarkable, so how to further improve the performance of the polyacrylonitrile-based carbon fibers is always the key point and the difficulty of carbon fiber technology development.
The carbon fiber weightlessness in the low-temperature carbonization process is generally more than 40%, non-carbon elements O, H, N in the fiber are largely escaped, the weightless fiber is changed from a solid state to a gaseous state, a large amount of pyrolysis gas is generated, and generated waste gas and tar are not discharged timely, so that the fiber running in a furnace chamber is polluted, local defects are generated, even the fiber running in the high-temperature carbonization process is caused to generate larger defects, the running period of a production line is shortened due to accumulation of tar, and the running cost of the production line is indirectly increased. Therefore, the instantaneous waste discharge of the low-temperature carbonization furnace is usually the key point of the structural design and process adjustment of the low-temperature furnace. With quality improvement and synergy as starting points, the single-line productivity of the carbon fiber is steadily improved, and the higher requirement on the waste capacity of the low-temperature grate is also provided. In addition, there is a contradiction point in the low-temperature carbonization process control, in order to reduce the adverse effect of waste gas and tar on the filament bundles, the exhaust gas discharge capacity needs to be increased as much as possible, but with the improvement of the exhaust gas discharge capacity, the gas sealing effect of the furnace tail of the furnace head can be greatly reduced, even oxygen is introduced into the furnace to cause the rapid reduction of the carbon fiber performance, and in the daily process adjustment process, a long time is often required to find the balance point of the low-temperature carbonization state, which is time-consuming and labor-consuming and is unfavorable for the improvement of the stability of the product performance.
The low-temperature carbonization process (usually between 300 and 1000 ℃) is mainly thermal decomposition reaction, the high-temperature carbonization process (usually between 1000 and 1500 ℃) is mainly thermal polycondensation reaction, and the process draft multiplying power is also different, so that the low-temperature carbonization furnace and the high-temperature carbonization furnace are usually of split type design, an operation area of 3 to 5 meters is usually reserved between the low-temperature furnace and the high-temperature furnace in actual production process, and the high-temperature fiber (usually more than 150 ℃) at the outlet of the low-temperature furnace absorbs water vapor in the air during the operation process of the area (usually about 1 to 5 minutes) and brings the water vapor into the high-temperature furnace. Although most of the water vapor in the tow band is blown out by the furnace mouth gas seal or discharged along with the high Wen Lutou waste discharge pipeline, a part of the water vapor is still carried into the furnace chamber and combined with carbon atoms on the fibers and used as CO+H in the high-temperature carbonization process 2 Or CO, resulting in the creation of defects such as fiber voids and even holes. The Chinese patent application (CN 107881599A) also describes that the environmental water vapor is easy to generate the adverse effect of the defect of the high-temperature carbonization process, and also provides a method for adding a constant temperature and constant humidity chamber among the pre-oxidation furnace, the low-temperature carbonization furnace and the high-temperature carbonization furnace. However, the method is considered to establish a constant temperature and humidity chamber in a region with large heat radiation in a high and low temperature furnace region, and although the method reduces the influence of the environmental humidity on the fiber to a certain extent, the method has high construction and maintenance cost, and once gas leakage such as HCN, NH3 and the like occurs, the method is closedThere is also a certain safety risk for operators in the space.
Disclosure of Invention
The invention aims to provide a preparation method of polyacrylonitrile-based carbon fiber with low structural defects.
In order to solve the problems and provide a preparation method of polyacrylonitrile-based carbon fiber with low structural defects, the technical scheme provided by the invention is as follows:
a preparation method of polyacrylonitrile-based carbon fiber with low structural defects comprises the steps of unwinding a precursor, sequentially carrying out the procedures of pre-oxidation, low-temperature carbonization, high-temperature carbonization, surface treatment, water washing, sizing, drying and winding carbonization to obtain the finished carbon fiber.
The invention arranges the low-temperature carbonization furnace of the high-efficiency coke discharging system, more instantaneously and efficiently discharges the low-temperature carbonized waste gas out of the furnace chamber, and reduces the damage of byproducts such as tar and the like to fibers.
The high-temperature carbonization furnace is provided with the filament bundle dehumidifying device, so that the damage of water vapor to fibers in the high-temperature carbonization process is reduced.
Compared with the prior art, the invention has the remarkable advantages that:
(1) The invention provides the low-temperature carbonization furnace of the efficient coke discharging system, which can discharge the low-temperature carbonized waste gas out of the furnace chamber more instantaneously and efficiently, thereby reducing the damage of byproducts such as tar and the like to fibers;
(2) The novel filament bundle dehumidifying device matched with the high-temperature carbonization furnace reduces the damage of water vapor to fibers in the high-temperature carbonization process and reduces the defects in the high-temperature carbonization process;
(3) The invention further slows down and reduces the expansion and development of the defects of the fiber structure in the carbonization process through the fine adjustment of the drafting at each stage in the carbonization process.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a schematic view of a low temperature furnace of the present invention.
Wherein, 1: first airtight chamber (furnace end), 2: second atmoseal room (furnace end), 3: a blower; 4: nitrogen gas seal, 5: electric heating, 6: low temperature carbonization furnace, 7: the third air seal chamber (furnace tail), 8, a furnace tail water cooling system, 9 and a fourth air seal chamber (furnace tail); 10. waste pipes.
FIG. 2 shows a high temperature carbonization furnace with a filament bundle dehumidifying device according to the present invention.
Wherein, 11: tow dehumidifying device, 11-1: hot air duct, 12: high temperature furnace end gas seal, 13, high temperature furnace end exhaust pipeline, 14: high temperature furnace, 15: high temperature furnace water cooling system, 16: high Wen Lulu tail gas seal.
Detailed Description
The invention is further explained below with reference to examples.
A preparation method of polyacrylonitrile-based carbon fiber with low structural defects comprises the steps of unwinding a precursor, sequentially carrying out the procedures of pre-oxidation, low-temperature carbonization, high-temperature carbonization, surface treatment, water washing, sizing, drying and winding carbonization to obtain the finished carbon fiber.
As shown in FIG. 1, the low-temperature carbonization furnace used in the invention has the following specific structure: the first air seal chamber 1 (furnace end), the second air seal chamber 2 (furnace end), the low-temperature carbonization furnace 6, the third air seal chamber 7 (furnace tail) and the fourth air seal chamber 9 (furnace tail) are sequentially arranged; the second air sealing chamber 2 (furnace end) is provided with a nitrogen air seal 4 and an electric heater 5; the low-temperature carbonization furnace 6 is provided with a waste discharge pipeline 10, and the waste discharge pipeline 10 is connected with a fan 3; the third air seal chamber 7 is provided with a furnace tail water cooling system 8. The first air seal chamber 1 (furnace end) and the fourth air seal chamber 9 (furnace tail) are respectively provided with a channel connected with the fan 3.
As shown in FIG. 2, the high-temperature carbonization furnace provided with the filament bundle dehumidifying device has the following specific structure:
the device comprises a silk bundle dehumidifying device 11, a high-temperature furnace end gas seal 12, a high-temperature furnace 14 and a high Wen Lulu tail gas seal 16 which are sequentially arranged. Wherein, the filament bundle dehumidifying device 11 is provided with a hot air pipeline 11-1, a high temperature furnace end waste discharge pipeline 13 is arranged at the high temperature furnace end air seal 12, and a high temperature furnace water cooling system 15 is arranged at the high temperature furnace tail.
The method comprises the following specific steps:
(1) The precursor is prepared by dry-jet wet spinning, the strength of the filament is more than or equal to 7.0cN/dtex, and the fineness is 0.50-0.70 dtex; after unwinding, the raw yarn sequentially passes through three independent temperature control devicesThe preoxidation furnace is respectively at the temperature of 200-300 ℃, and the temperature control precision of the effective heating area of the single preoxidation furnace is within +/-2 ℃; the filament bundles in the furnaces are drafted to different degrees by independent driving between each oxidation furnace, and the total draft ratio is-12 to +5%; controlling the density of the preoxidized body as a quantitative index for evaluating the preoxidation degree, wherein the control range of the density of the preoxidized body is 1.340-1.360 g/cm 3 Between them.
(2) The pre-oxidized fiber bundles pass through a low-temperature carbonization furnace provided with a high-efficiency coke discharging system, wherein the pressure difference between a first air sealing chamber and a second air sealing chamber is 1-10 Pa, the highest heating temperature in the second air sealing chamber of a furnace end is 400 ℃, a water cooling device is arranged in the second air sealing chamber of a furnace tail, and the temperature of an outlet fiber of the low-temperature furnace is controlled to be not more than 150 ℃; the low-temperature carbonization furnace is divided into 6-8 heating temperature areas, the carbonization temperature is 300-1000 ℃, and the heating rate is about 40-100 ℃/min; the low-temperature carbonization draft rate is controlled by the front-back driving speed ratio of the low-temperature furnace, and the draft rate is +1 to +5 percent.
(3) The low-carbon filament bundles subjected to low-temperature carbonization firstly pass through a filament bundle dehumidifying device and then enter a high-temperature carbonization furnace. The gap between the filament bundle dehumidifying device and the furnace mouth of the high-temperature furnace is 5-50 mm, so that moisture on the filament bundle is not brought into the high-temperature furnace after escaping, the height of the inner cavity of the filament bundle dehumidifying device is about 5-30 mm, the heating mode is that the middle is blown by hot air from two ends, the temperature of the hot air is 110-150 ℃, the air heating can be carried out by utilizing the heat exchanged by the low-temperature carbonization furnace, and the air speed of the hot air is not more than 5m/s; the high-temperature carbonization furnace head is provided with a nitrogen gas seal and a waste discharge pipeline, the furnace tail is provided with a water cooling system, and the temperature of an outlet wire of the high-temperature furnace is controlled to be not more than 150 ℃; the high-temperature carbonization furnace is divided into 4-8 heating temperature areas, the carbonization temperature is 1000-1600 ℃, and the heating rate is about 100-150 ℃/min; the high-temperature carbonization draft rate is controlled by the front-back driving speed ratio of the high-temperature furnace, and the draft rate is-8 to-2 percent.
(4) The high-carbon filament bundles carbonized at high temperature are subjected to one-to-two-stage surface treatment in a surface treatment tank, and the surface treatment electrolyte is preferably ammonium salt electrolytes such as ammonium bicarbonate, ammonium dihydrogen phosphate, ammonium sulfate and the like; the surface treatment electric quantity is set according to the application requirement, and is preferably 1-50 c/g; and washing and drying the tows subjected to surface treatment.
(5) The tows subjected to surface treatment and water washing are continuously subjected to sizing through a sizing tank, sizing agents are preferably epoxy resin sizing agents, and the concentration of the sizing agents is preferably 0.5-1.5%; and drying the sized tows in a drying furnace at about 150 ℃ to obtain a carbon fiber finished product by winding.
And finally, quantitatively evaluating the sizes and the distribution of pores or holes on the carbon fiber by adopting a small-angle X-ray diffraction method.
Different sets of experiments were performed in combination with the above methods, and the specific data are as follows:
description:
comparative example 1, blank control group
Comparative example 2, compared with comparative example 1, the low temperature furnace waste discharge is increased, the low temperature furnace is sealed by two chambers of negative pressure, the furnace body is charged with oxygen, the micropore volume is increased, and the strength is reduced
Comparative example 3, only the first chamber and the second chamber of the low-temperature furnace are matched, the waste discharge capacity is improved, the micropore volume is reduced, and the strength is improved; no high temperature dehumidification
Example 1, on the basis of comparative example 3, high temperature dehumidification was added, micropore volume was further reduced, and strength was improved
Example 2 based on example 1, the pressure of the low temperature seal chamber was adjusted, the micropore volume was decreased, and the strength was improved
Example 3 based on example 2, the pressure of the low temperature seal chamber was adjusted, the high temperature dehumidification was adjusted, the micropore volume was decreased, and the strength was improved
Example 4 based on example 3, the pressure of the low temperature seal chamber was adjusted, the high temperature dehumidification was adjusted, and the fine adjustment of pre-oxidation, low temperature carbonization and high temperature carbonization draft during carbonization (i.e., adjustment of carbonization process) was further adjusted, the micropore volume was decreased, and the strength was improved
Example 5 based on example 4, the pressure of the low temperature seal chamber was adjusted, the high temperature dehumidification was adjusted, the micropore volume was increased, and the strength was decreased
In example 6, the pressure of the low-temperature seal chamber was adjusted based on example 5, the carbonization process was adjusted, the micropore volume was increased, and the strength was decreased.
Claims (8)
1. A preparation method of polyacrylonitrile-based carbon fiber with low structural defects is characterized by comprising the following steps: the method comprises the following steps:
preparing a dry-jet wet spinning preparation precursor, wherein the strength of the filament is more than or equal to 7.0cN/dtex, and the fineness is 0.50-0.70 dtex;
after the precursor is unreeled, the precursor sequentially passes through a plurality of independent temperature control pre-oxidation furnaces, and tows in the furnaces are subjected to different degrees of drafting by independent driving between each oxidation furnace, wherein the total drafting ratio is-12 to +5%; the density of the pre-oxidized fiber body is controlled within the range of 1.340-1.360 g/cm 3 Between them;
the pre-oxidized fiber bundles pass through a low-temperature carbonization furnace with a two-stage gas seal chamber structure, wherein the furnace end and the furnace tail of the low-temperature carbonization furnace are respectively provided with two-stage gas seal chambers, the pressure difference between the first-stage gas seal chamber and the second-stage gas seal chamber of the two-stage gas seal chambers is 1-10 Pa, the highest heating temperature in the second-stage gas seal chamber of the furnace end is 400 ℃, the second-stage gas seal chamber of the furnace tail is provided with a water cooling device, and the outlet fiber temperature of the low-temperature furnace is controlled to be not more than 150 ℃; controlling the low-temperature carbonization draft rate by the front-back driving speed ratio of the low-temperature furnace, wherein the draft rate is +1- +5%;
the low-carbon tows subjected to low-temperature carbonization pass through a high-temperature carbonization furnace provided with a tows dehumidifying device, and the high-temperature carbonization draft rate is controlled by driving a speed ratio back and forth through the high-temperature furnace, wherein the draft rate is-8 to-2%;
the high-carbon tows subjected to high-temperature carbonization are subjected to one-to-two-stage surface treatment in a surface treatment tank, and the tows subjected to surface treatment are washed and dried;
and (3) sizing the surface-treated and water-washed tows continuously through a sizing tank, and drying the sized tows at 150 ℃ to obtain a carbon fiber finished product by winding.
2. The method for preparing the polyacrylonitrile-based carbon fiber with low structural defects according to claim 1, wherein the method comprises the following steps: the preoxidation temperature of the temperature-controlled preoxidation furnace is between 200 and 300 ℃, and the temperature control precision of the effective heating area of the single preoxidation furnace is within +/-2 ℃.
3. The method for preparing the polyacrylonitrile-based carbon fiber with low structural defects according to claim 1, wherein the method comprises the following steps: the two-stage gas seal chamber structure of the low-temperature carbonization furnace is characterized in that a fan is connected in a first-stage gas seal chamber, an air outlet of the fan is connected with a low-temperature furnace waste gas treatment system, and the pressure difference between the first-stage gas seal chamber and a second-stage gas seal chamber is kept at 1-10 Pa; the secondary air seal chamber of the furnace end is provided with a heating device, and the heating temperature is 150-400 ℃.
4. The method for preparing the polyacrylonitrile-based carbon fiber with low structural defects according to claim 1, wherein the method comprises the following steps: the low-temperature carbonization furnace is divided into 6-8 heating temperature areas, the carbonization temperature is 300-1000 ℃, and the heating rate is 40-100 ℃/min.
5. The method for preparing the polyacrylonitrile-based carbon fiber with low structural defects according to claim 1, wherein the method comprises the following steps: the high-temperature carbonization furnace provided with the filament bundle dehumidifying device is characterized in that a gap of 5-50 mm is reserved between the filament bundle dehumidifying device and a furnace mouth of the high-temperature furnace, so that moisture on filament bundles can not be brought into the high-temperature furnace after escaping; the height of the inner cavity of the filament bundle dehumidifying device is 5-30 mm, the heating mode is that the middle is purged by hot air towards the two ends, the temperature of the hot air is 110-150 ℃, the air heating can be carried out by utilizing the heat exchanged by the low-temperature carbonization furnace, and the air speed of the hot air is not more than 5m/s; the furnace end of the high-temperature carbonization furnace is provided with an air seal and a waste discharge pipeline, the furnace tail is provided with a water cooling system, and the temperature of outlet wires of the high-temperature carbonization furnace is controlled to be not more than 150 ℃.
6. The method for preparing the polyacrylonitrile-based carbon fiber with low structural defects according to claim 1 or 5, wherein the method comprises the following steps: the high-temperature carbonization furnace is divided into 4-8 heating temperature areas, the carbonization temperature is 1000-1600 ℃, and the heating rate is 100-150 ℃/min.
7. The method for preparing the polyacrylonitrile-based carbon fiber with low structural defects according to claim 1, wherein the method comprises the following steps: the surface treatment electrolyte is ammonium salt electrolyte of ammonium bicarbonate, ammonium dihydrogen phosphate and ammonium sulfate; the surface treatment electric quantity is set according to the application requirement, and is specifically 1-50 c/g.
8. The method for preparing the polyacrylonitrile-based carbon fiber with low structural defects according to claim 1, wherein the method comprises the following steps: the sizing agent is epoxy resin sizing agent, and the concentration of the sizing agent is 0.5-1.5%.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111415584.5A CN114481366B (en) | 2021-11-25 | 2021-11-25 | Preparation method of low-defect polyacrylonitrile-based carbon fiber |
| PCT/CN2022/134204 WO2023093823A1 (en) | 2021-11-25 | 2022-11-25 | Preparation method for low-defect polyacrylonitrile-based carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111415584.5A CN114481366B (en) | 2021-11-25 | 2021-11-25 | Preparation method of low-defect polyacrylonitrile-based carbon fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114481366A CN114481366A (en) | 2022-05-13 |
| CN114481366B true CN114481366B (en) | 2023-08-04 |
Family
ID=81492369
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111415584.5A Active CN114481366B (en) | 2021-11-25 | 2021-11-25 | Preparation method of low-defect polyacrylonitrile-based carbon fiber |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN114481366B (en) |
| WO (1) | WO2023093823A1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114481366B (en) * | 2021-11-25 | 2023-08-04 | 中复神鹰碳纤维股份有限公司 | Preparation method of low-defect polyacrylonitrile-based carbon fiber |
| CN114892313B (en) * | 2022-06-14 | 2023-06-27 | 山西钢科碳材料有限公司 | Method for loading polyacrylonitrile fibers into carbon fibers |
| CN115434042B (en) * | 2022-09-23 | 2023-10-03 | 山西钢科碳材料有限公司 | Atmosphere control method for polyacrylonitrile-based carbon fiber pre-oxidized fiber in carbonization process |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4314981A (en) * | 1978-12-26 | 1982-02-09 | Jureha Kagaku Kogyo Kabushiki Kaisha | Method for preparing carbon fibers |
| CN201280433Y (en) * | 2008-03-26 | 2009-07-29 | 威海拓展纤维有限公司 | Low-temperature carbonization furnace with dehumidifier |
| CN103882560A (en) * | 2014-04-07 | 2014-06-25 | 北京化工大学 | Online dehumidification and deoxidation device for continuous production of carbon fibers |
| KR20140130612A (en) * | 2013-05-01 | 2014-11-11 | 주식회사 뉴파워 프라즈마 | Heat treatment apparatus for carbon fiber manufacture and carbon fiber manufacture system with the same |
| CN207031623U (en) * | 2017-07-04 | 2018-02-23 | 浙江精功科技股份有限公司 | A kind of polyacrylonitrile-based carbon fibre low-carbon sealing gland high temperature nitrogen blow device |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190048493A1 (en) * | 2017-08-14 | 2019-02-14 | Ching-Long Ong | Carbon fiber bundle forming device and method |
| CN114481366B (en) * | 2021-11-25 | 2023-08-04 | 中复神鹰碳纤维股份有限公司 | Preparation method of low-defect polyacrylonitrile-based carbon fiber |
-
2021
- 2021-11-25 CN CN202111415584.5A patent/CN114481366B/en active Active
-
2022
- 2022-11-25 WO PCT/CN2022/134204 patent/WO2023093823A1/en unknown
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4314981A (en) * | 1978-12-26 | 1982-02-09 | Jureha Kagaku Kogyo Kabushiki Kaisha | Method for preparing carbon fibers |
| CN201280433Y (en) * | 2008-03-26 | 2009-07-29 | 威海拓展纤维有限公司 | Low-temperature carbonization furnace with dehumidifier |
| KR20140130612A (en) * | 2013-05-01 | 2014-11-11 | 주식회사 뉴파워 프라즈마 | Heat treatment apparatus for carbon fiber manufacture and carbon fiber manufacture system with the same |
| CN103882560A (en) * | 2014-04-07 | 2014-06-25 | 北京化工大学 | Online dehumidification and deoxidation device for continuous production of carbon fibers |
| CN207031623U (en) * | 2017-07-04 | 2018-02-23 | 浙江精功科技股份有限公司 | A kind of polyacrylonitrile-based carbon fibre low-carbon sealing gland high temperature nitrogen blow device |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2023093823A1 (en) | 2023-06-01 |
| CN114481366A (en) | 2022-05-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114481366B (en) | Preparation method of low-defect polyacrylonitrile-based carbon fiber | |
| CN103046165B (en) | Preparation method of continuous filament of asphalt-based carbon fiber | |
| CN110055624B (en) | Pre-oxidation method of polyacrylonitrile fiber, polyacrylonitrile carbon fiber and preparation method | |
| US20060257720A1 (en) | Conductive carbonaceous fiber woven cloth and solid polymer-type fuel cell | |
| CN101956251B (en) | High-temperature furnace sealing device for continuously producing carbon fibres | |
| CN211522400U (en) | Microwave heating carbon fiber precursor annealing-pre-oxidation treatment equipment | |
| CN108203848A (en) | A kind of hot high modulus pitch-based carbon fiber of high-strength highly-conductive and preparation method thereof | |
| CN111118671B (en) | Preparation method of 25k large-tow carbon fiber | |
| CN103882560A (en) | Online dehumidification and deoxidation device for continuous production of carbon fibers | |
| CN111020750B (en) | High-speed preparation method for producing large-tow carbon fibers | |
| CN103696232A (en) | Activation technology for producing activated carbon fibers | |
| CN108239801A (en) | A kind of big tow asphalt base carbon fiber and preparation method thereof | |
| CN202116703U (en) | Drying device for fiber beam spinning | |
| CN108286088A (en) | A kind of asphalt base carbon fiber and preparation method thereof that can be used for weaving | |
| CN109957860A (en) | The preparation method of viscose glue pyrographite carbon fiber | |
| CN110846744A (en) | Method for regulating and controlling homogenization of carbon fiber pre-oxidized fiber and pre-oxidation furnace | |
| CN116024701A (en) | Polyacrylonitrile-based large-tow carbon fiber and preparation method thereof | |
| CN107881599B (en) | Method for improving strength of polyacrylonitrile-based carbon fiber | |
| CN108360147A (en) | A method of preparing the pre- oxygen felt of polyacrylonitrile | |
| CN114457463B (en) | Large-tow carbon fiber preoxidation furnace and preoxidation method | |
| CN116377619A (en) | 35-50K carbon fiber, preparation method thereof and pre-oxidation furnace for producing 35-50K carbon fiber | |
| CN100339523C (en) | Microwave thermal reaction device for carbonizing pre-oxidized fiber, and processing technique | |
| CN115467049B (en) | Carbon fiber rotary vertical air path pre-oxidation furnace | |
| CN115744881B (en) | Catalyst for ultralow-temperature growth of carbon nano tube on surface of continuous carbon fiber and application thereof | |
| CN115449925A (en) | Preparation system and method for graphitizing polyacrylonitrile carbon fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |